建立了快速测定水产加工食品中河豚毒素(tetrodotoxin,TTX)的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。样品经0.1%乙酸水溶液提取,C18萃取剂分散固相萃取净化,超滤管过滤后进行分析。目标物TYX采用TSK-gelAmide-80亲水色谱柱进行分离,以电喷雾离子源、多反应监测(MRM)正离子模式检测,基质标准曲线校正,外标法定量。结果表明,TTX在2-200ng/mL范围内线性良好(r^2〉0.999),方法的定量限为10μg/kg,加标回收率为71.2%~102%,相对标准偏差(RSD)为5.23%-12.4%。方法操作简便,准确度和精密度良好,可用于烤鱼片、鱼干等干制水产加工食品中河豚毒素的测定,具有较好的应用价值。
A method for the rapid determination of tetrodotoxin (TTX) in aquatic food using ultra performance liquid chromatography- tandem mass spectrometry( UPLC -MS/MS) has been established. TTX was extracted from sample by 0.1% acetic acid -water, and then purified by dispersive solid -phase extraction with Cls extraction sorbent and filtered through a Mr 10000 cut - off ultrafree microcentrifuge filter. The separation of TYX was carried out on a col- umn of TSK - gel Amide - 80, and detected by positive electrospray ionization tandem mass spectrometry in the MRM mode. The matrix- matched external standard calibration curves were used for quantitative analysis. The calibration curves were linear in the range of 2 - 200 ng/mL for TI'X, with quantification limit of 10 μg/kg. The average recover- ies were between 71.2% and 102% with relative standard deviations(RSD) ranging from 5.23% to 12.4%. The proposed method was simple, rapid, accurate and applicable for the determination of TTX in aquatic food.